CN109735807A - A kind of preparation method of negative temperature coefficient heat-sensitive film - Google Patents
A kind of preparation method of negative temperature coefficient heat-sensitive film Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of negative temperature coefficient heat-sensitive film, comprising the following steps: (1) cleaning of substrate；(2) prepared by thermosensitive film: Mn-Co-Ni alloy target material being splashed on substrate using magnetron sputtering method and obtains Mn-Co-Ni system film；(3) it makes annealing treatment: Mn-Co-Ni system film being subjected to anneal oxidation processing under the atmosphere containing oxygen, Mn-Co-Ni-O series negative temperature coefficient thermosensitive film can be obtained.The present invention passes through to preparation method overall flow technological design, target material used by especially crucial sputtering technology improves, using Mn-Co-Ni system alloy as target, it can effectively solve the problem that the problem that ceramic target is easy to break when magnetron sputtering method prepares thermosensitive film, utilization rate is low compared with prior art, preparation method is easy to operate, it is easy to accomplish, it is reproducible.
Description
Technical field
The invention belongs to informational function ceramic membrane preparation technical fields, more particularly, to a kind of negative temperature system
The preparation method of number thermosensitive film, the thermosensitive film especially Mn-Co-Ni-O, Mn-Ni-O and Mn-Fe-Ni-O series negative temperature
Coefficient (NTC) thermosensitive film.
Background technique
Negative temperature coefficient (NTC) thermo-sensitive material refers to its resistance value electronic material reduced with the raising of temperature.NTC heat
Quick resistance is due to high sensitivity, stability is good, lower-price characteristic, is widely used in temperature sensor, household electrical appliance, red
The fields such as outer detection.By taking Mn-Co-Ni-O based material as an example, there is spinelle (AB2O4) structure Mn-Co-Ni-O based material by
In showing excellent negative temperature coefficient and preferable stability, become presently the most common NTC thermistor material it
One.Compared with traditional block, thick-film thermistor, thin-film material (thickness is generally less than 10 microns) can satisfy semiconductor row
The miniaturization of industry product and integrated demand, and have many advantages, such as high sensitivity, respond it is fast, MEMS, integrated circuit with
And the fields such as micro-nano device have broad application prospects, and have very high practical value and economic value.
The method for preparing NTC thermosensitive film at present mainly has magnetron sputtering method, evaporation coating method, metallorganic thermal decomposition
Method, pulsed laser deposition etc..The Kukuruznyak Dmitry of Washington, DC university in 2006 metallorganic heat point
Solution is prepared for Ni0.48Co0.24Cu0.6Mn1.68O4Film (Moyer, Jerome G, Kukuruznyak, Dmitry A, et
al.Thermopower and electrical conductivity of Mn1.68-XCu0.6+X+Y+ZCo0.24-YNi0.48-Z thin
film oxides obtained through metal organic decomposition processing[J]
.JOURNAL OF APPLIED PHYSICS, 2006,100 (8), 083514.), what domestic woods et al. is in the patent with metal
Solution decomposition method is prepared for Mn-Co-Ni-O/Mn-Co-Ni-Cu-O/Mn-Co-Ni-O Sandwich film (Chinese patent ZL
The characteristics of 2015 10143370.5), this method are that condition controllability is good, but prepared film composition and thickness can be uneven
It is even.R.Schmidt in 2001 and
A.W.Brinkman deposited by electron beam evaporation method is prepared for NiMn2O4Film (Schmidt R, Brinkman A
W.Preparation and characterization of NiMn2O4films[J].Int J Inorg Mater,2001,
3,1215-1217.), but this method is unable to control NiMn2O4The film deposition process that raw material are decomposed and reconfigured.Always
The advantages of evaporation coating method is that equipment is simple for body, easy to operate, and film forming speed is fast, high-efficient, can be obtained clearly with mask
Clear figure.The disadvantage is that film and substrate adhesive force are weaker, high-melting-point substances being difficult to be evaporated, process repeatability is not good enough,
And it is not easy to guarantee exact composition of material etc..M.H.Lee and M.N.Yoo in 2002 et al. is prepared for pulse laser deposition
Mn1.5CoNi0.5O4Thermosensitive film (Lee M H, Yoo M N.Detectivity of thin film NTC thermal
Sensors [J] .Sens Actuat A, 2002,96 (1), 97-104.), the characteristics of this method prepares film is deposition velocity
Fastly, depositing temperature is low, and the film of preparation is uniform, but equipment is expensive.The method system that A.Basu et al. passes through rf magnetron sputtering
For NixMn3-xO4+δ(0.4≤x≤1.0) film (Basu A, Brinkman A W, Klusek Z, et al.In situ
study of the effect of temperature on the electronic structure of NixMn3-xO4+δ
thin films using scanning tunneling spectroscopy[J].J Appl Phys,2002,92(7),
4123-4125.), this method preparation crystalline property is good, with high purity, good evenness, and film is preferable with substrate in conjunction with,
It is easy to be mass produced, but traditional ceramic target utilization rate easy to break is low.
To solve the above-mentioned problems, the present invention proposes the method for sputtering then anneal oxidation in air using alloy target material
Mn-Co-Ni-O thermosensitive film is prepared, prepared film equally has spinel structure, and surface particularly compact, is conducive to
Reduce room temperature resistance.
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, the purpose of the present invention is to provide a kind of negative temperature coefficient heat
The preparation method of sensitive film, wherein by preparation method overall flow technological design, especially crucial sputtering technology is used
Target material improve, for preparing Mn-Co-Ni-O system film, using Mn-Co-Ni system alloy as target, use first
Mn-Co-Ni alloy target material sputters a laminated gold thin film on an insulating substrate, and then alloy firm is put into such as air furnace and is moved back
Fire oxidation, to prepare with spinel structure, and the NTC thermosensitive film of surface compact is (that is, Mn-Co-Ni-O system subzero temperature
Spend coefficient heat-sensitive film).It can effectively solve the problem that ceramic target holds when magnetron sputtering method prepares thermosensitive film compared with prior art
The low problem of easy fragmentation, utilization rate, preparation method of the present invention is easy to operate, easy to accomplish, reproducible, and is closed by regulation
The specific type and proportion of the metallic element of alloying component in gold target material, are applicable to various proportions and different metal element is mixed
Miscellaneous NTC thermosensitive film.
To achieve the above object, according to one aspect of the present invention, a kind of system of negative temperature coefficient heat-sensitive film is provided
Preparation Method, which comprises the following steps:
(1) cleaning of substrate；
(2) prepared by thermosensitive film: after Mn-Co-Ni alloy target material is splashed to step (1) cleaning using magnetron sputtering method
On the substrate of resulting drying, Mn-Co-Ni system film is obtained；Wherein, condition used by the sputtering are as follows: basic air pressure <
1x10-4Pa, sputter gas are the high-purity Ar gas that purity is not less than 99.9%, and sputtering power meets 80-120W, and underlayer temperature is
100-250℃；
(3) it makes annealing treatment: the resulting Mn-Co-Ni system film of step (2) is subjected to annealing oxygen under the atmosphere containing oxygen
Mn-Co-Ni-O system film is prepared in change processing, the Mn-Co-Ni-O system film, that is, Mn-Co-Ni-O series negative temperature coefficient temperature-sensitive
Film；Wherein, it is 600-900 DEG C that the anneal oxidation, which handles used annealing temperature, and soaking time of annealing is 90-150 points
Clock.
As present invention further optimization, in the step (2), described its alloying component of Mn-Co-Ni alloy target material
Mainly it is made of Mn element, Co element and Ni element.
As present invention further optimization, in the step (2), described its alloying component of Mn-Co-Ni alloy target material
It is made of Mn element, Co element and Ni element；Correspondingly, Mn-Co-Ni-O system film made from the step (3) is specific
For Mn-Co-Ni-O film.
As present invention further optimization, in the step (2), described its alloying component of Mn-Co-Ni alloy target material
In further include Cu element, correspondingly, Mn-Co-Ni-O system film made from the step (3) is specially Mn-Co-Ni-Cu-
O film.
As present invention further optimization, in the step (3), anneal oxidation processing be in air atmosphere into
Capable.
As present invention further optimization, the preparation method of the negative temperature coefficient heat-sensitive film further includes following step
It is rapid:
(4) electrode is prepared: the Mn-Co-Ni-O system film obtained using the method for evaporation coating in the step (3)
Surface prepares interdigital electrode.
It is another aspect of this invention to provide that the present invention provides a kind of preparation method of negative temperature coefficient heat-sensitive film,
It is characterized in that, comprising the following steps:
(1) cleaning of substrate；
(2) prepared by thermosensitive film: Mn-Ni alloy target material being splashed to institute after step (1) is cleaned using magnetron sputtering method
On the substrate of the drying obtained, Mn-Ni system film is obtained；Wherein, condition used by the sputtering are as follows: basic air pressure < 1x10- 4Pa, sputter gas are the high-purity Ar gas that purity is not less than 99.9%, and sputtering power meets 80-120W, underlayer temperature 100-
250℃；
(3) it makes annealing treatment: the resulting Mn-Ni system film of step (2) is subjected to anneal oxidation under the atmosphere containing oxygen
Mn-Ni-O system film is prepared in processing, the Mn-Ni-O system film, that is, Mn-Ni-O series negative temperature coefficient thermosensitive film；Wherein,
It is 600-900 DEG C that the anneal oxidation, which handles used annealing temperature, and annealing soaking time is 90-150 minutes.
Another aspect according to the invention, the present invention provides a kind of preparation method of negative temperature coefficient heat-sensitive film,
It is characterized in that, comprising the following steps:
(1) cleaning of substrate；
(2) prepared by thermosensitive film: after Mn-Fe-Ni alloy target material is splashed to step (1) cleaning using magnetron sputtering method
On the substrate of resulting drying, Mn-Fe-Ni system film is obtained；Wherein, condition used by the sputtering are as follows: basic air pressure <
1x10-4Pa, sputter gas are the high-purity Ar gas that purity is not less than 99.9%, and sputtering power meets 80-120W, and underlayer temperature is
100-250℃；
(3) it makes annealing treatment: the resulting Mn-Fe-Ni system film of step (2) is subjected to annealing oxygen under the atmosphere containing oxygen
Mn-Fe-Ni-O system film is prepared in change processing, the Mn-Fe-Ni-O system film, that is, Mn-Fe-Ni-O series negative temperature coefficient temperature-sensitive
Film；Wherein, it is 600-900 DEG C that the anneal oxidation, which handles used annealing temperature, and soaking time of annealing is 90-150 points
Clock.
Contemplated above technical scheme through the invention, compared with prior art, to prepare Mn-Co-Ni-O system film
For, due to being used as target using Mn-Co-Ni system alloy, by control target for alloy phase, elder generation utilizes the target on substrate
Material carry out sputter process obtain alloy-layer (and, it is particularly possible to by the element composition and ratio of target, obtain containing specific mesh
Mark metal species and the expected alloy-layer substantially matched), it then handles to obtain the subzero temperature of supplement oxygen element by anneal oxidation again
Spend coefficient heat-sensitive film.The preparation method of Mn-Co-Ni-O series negative temperature coefficient thermosensitive film, solves magnetic control and splashes in the present invention
Ceramic target utilization rate easy to break low technical problem when the method for penetrating prepares thermosensitive film.This method be suitable for it is various proportion and
The Mn-Co-Ni-O system NTC thermosensitive film of different element dopings, to the industrial mass of Mn-Co-Ni-O system NTC thermosensitive film
Production provides technical solution.
In the preparation of negative temperature coefficient heat-sensitive thin-film material, since negative temperature coefficient heat-sensitive thin-film material is usually Mn-
Co-Ni-O system film, Mn-Ni-O system film, Mn-Fe-Ni-O system film, compared to the prior art in the ceramic target that generallys use
Material, when using traditional ceramics target as sputter, target using after several times will fragmentation, utilization rate it is low, and can go out in sputtering process
Existing clast drops on substrate the quality for influencing film；And the present invention is by using the target of alloy phase (such as Mn-Co-Ni system alloy phase)
Material, these alloy target materials can be made by means such as alloy hot pressing, substitute traditional ceramics target in sputtering, target is not allowed
It is frangible, the preparation that equally can be realized negative temperature coefficient heat-sensitive thin-film material is reoxidized after sputtering, reaches same effect.
Detailed description of the invention
Fig. 1 is that (MCNO layer therein is to represent Mn-Co-Ni-O for the structural schematic diagram of NTC thermosensitive film prepared by the present invention
It is thermosensitive film).
Fig. 2 is the XRD spectrum of the Mn-Co-Ni-O thermosensitive material film prepared in embodiment 1.
Fig. 3 is the SEM figure of the Mn-Co-Ni-O thermosensitive material film prepared in embodiment 1.
Fig. 4 is the resistance-temperature relationship figure of the Mn-Co-Ni-O thermosensitive film element prepared in embodiment 1.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Not constituting a conflict with each other can be combined with each other.
Embodiment 1
A. the cleaning of substrate: first by the SiO of purchase2/ Si substrate, which is put into toluene solution, to be cleaned by ultrasonic 10 minutes, then is put
Enter to be cleaned by ultrasonic in acetone soln 10 minutes, then with being cleaned by ultrasonic 10 minutes in deionized water, place into dehydrated alcohol water
Ultrasonic cleaning 10 minutes, finally dries up substrate.
B. prepared by thermosensitive film: using magnetron sputtering method by Mn1.56Co0.96Ni0.48Alloy target material is splashed to obtained by step a
Substrate on, sputtering condition are as follows: basic air pressure 6x10-4Pa, operating air pressure 2Pa, (purity is not less than sputter gas high-purity Ar gas
99.9%), sputtering power 100W, 150 DEG C of underlayer temperature.Wherein, basic air pressure i.e. start sputtering before be passed through not yet argon gas it
Preceding air pressure.
C. it makes annealing treatment: the Mn-Co-Ni film that step b is obtained is put into high-temperature electric resistance furnace, be arranged 750 DEG C of temperature, heat preservation
Time 120 minutes, heating and rate of temperature fall were all 5 DEG C/min, obtained Mn-Co-Ni-O film.
D. prepared by electrode: using the method for evaporation coating in the silver-plated interdigital electrode of Mn-Co-Ni-O film surface.Interdigital length
Degree is 6.2mm, width 0.8mm.
The room temperature resistance R25 for measuring Mn-Co-Ni-O thermosensitive film in the embodiment is 71.1k Ω, and temperature-sensitive constant B value is
3306K。
Embodiment 2
A. the cleaning of substrate: first by the Al of purchase2O3Substrate, which is put into toluene solution, to be cleaned by ultrasonic 10 minutes, is placed into
It is cleaned by ultrasonic in acetone soln 10 minutes, then with being cleaned by ultrasonic 10 minutes in deionized water, places into dehydrated alcohol water and surpass
Sound cleans 10 minutes, finally dries up substrate.
B. prepared by thermosensitive film: using magnetron sputtering method by Mn1.56Co0.96Ni0.48Alloy target material is splashed to obtained by step a
Substrate on, sputtering condition are as follows: basic air pressure 6x10-4Pa, operating air pressure 2Pa, sputter gas high-purity Ar gas, sputtering power 80W,
100 DEG C of underlayer temperature.
C. it makes annealing treatment: the Mn-Co-Ni film that step b is obtained is put into high-temperature electric resistance furnace, be arranged 850 DEG C of temperature, heat preservation
Time 150 minutes, heating and rate of temperature fall were all 5 DEG C/min, obtained Mn-Co-Ni-O film.
D. prepared by electrode: using the method for evaporation coating in the silver-plated interdigital electrode of Mn-Co-Ni-O film surface.Interdigital length
Degree is 6.2mm, width 0.8mm.
Measure the room temperature resistance R of Mn-Co-Ni-O thermosensitive film in the embodiment25For 108.2k Ω, temperature-sensitive constant B value is
3381K。
Embodiment 3
A. the cleaning of substrate: first by the SiO of purchase2/ Si substrate, which is put into toluene solution, to be cleaned by ultrasonic 10 minutes, then is put
Enter to be cleaned by ultrasonic in acetone soln 10 minutes, then with being cleaned by ultrasonic 10 minutes in deionized water, place into dehydrated alcohol water
Ultrasonic cleaning 10 minutes, finally dries up substrate.
B. prepared by thermosensitive film: using magnetron sputtering method by Mn1.56Co0.96Ni0.48Cu0.15Alloy target material is splashed to step a
On resulting substrate, sputtering condition are as follows: basic air pressure 8x10-4Pa, operating air pressure 2Pa, sputter gas high-purity Ar gas, sputtering power
120W, 150 DEG C of underlayer temperature.Then Mn-Co-Ni-Cu film is put into high-temperature electric resistance furnace, 700 DEG C of temperature, soaking time 120
Minute, heating and rate of temperature fall are all 5 DEG C/min, obtain Mn-Co-Ni-Cu-O film.
C. prepared by electrode: using the method for evaporation coating in the silver-plated interdigital electrode of Mn-Co-Ni-Cu-O film surface.It is interdigital
Length is 6.2mm, width 0.8mm.
Measure the room temperature resistance R of Mn-Co-Ni-Cu-O thermosensitive film in the embodiment25For 22.6k Ω, temperature-sensitive constant B value
For 3224K.
Embodiment 4
A. the cleaning of substrate: the SiO2/Si substrate of purchase is put into toluene solution is cleaned by ultrasonic 10 minutes first, then put
Enter to be cleaned by ultrasonic in acetone soln 10 minutes, then with being cleaned by ultrasonic 10 minutes in deionized water, place into dehydrated alcohol water
Ultrasonic cleaning 10 minutes, finally dries up substrate.
B. prepared by thermosensitive film: using magnetron sputtering method by Mn1.56Co0.96Ni0.48Alloy target material is splashed to obtained by step a
Substrate on, sputtering condition are as follows: basic air pressure 6x10-4Pa, operating air pressure 2Pa, sputter gas high-purity Ar gas, sputtering power
100W, 250 DEG C of underlayer temperature.
C. it makes annealing treatment: the Mn-Co-Ni film that step b is obtained is put into high-temperature electric resistance furnace, be arranged 800 DEG C of temperature, heat preservation
Time 150 minutes, heating and rate of temperature fall were all 5 DEG C/min, obtained Mn-Co-Ni-O film.
D. prepared by electrode: using the method for evaporation coating in the silver-plated interdigital electrode of Mn-Co-Ni-O film surface.Interdigital length
Degree is 6.2mm, width 0.8mm.
Measure the room temperature resistance R of Mn-Co-Ni-O thermosensitive film in the embodiment25For 103.2k Ω, temperature-sensitive constant B value is
3356K。
Embodiment 5
A. the cleaning of substrate: first by the SiO of purchase2/ Si substrate, which is put into toluene solution, to be cleaned by ultrasonic 10 minutes, then is put
Enter to be cleaned by ultrasonic in acetone soln 10 minutes, then with being cleaned by ultrasonic 10 minutes in deionized water, place into dehydrated alcohol water
Ultrasonic cleaning 10 minutes, finally dries up substrate.
B. prepared by thermosensitive film: using magnetron sputtering method by Mn1.56Co0.96Ni0.48Alloy target material is splashed to obtained by step a
Substrate on, sputtering condition are as follows: basic air pressure 6x10-4Pa, operating air pressure 2Pa, sputter gas high-purity Ar gas, sputtering power
100W, 250 DEG C of underlayer temperature.
C. it makes annealing treatment: the Mn-Co-Ni film that step b is obtained is put into high-temperature electric resistance furnace, be arranged 600 DEG C of temperature, heat preservation
Time 120 minutes, heating and rate of temperature fall were all 5 DEG C/min, obtained Mn-Co-Ni-O film.
D. prepared by electrode: using the method for evaporation coating in the silver-plated interdigital electrode of Mn-Co-Ni-O film surface.Interdigital length
Degree is 6.2mm, width 0.8mm.
Measure the room temperature resistance R of Mn-Co-Ni-O thermosensitive film in the embodiment25For 137.2k Ω, temperature-sensitive constant B value is
3365K。
Embodiment 6
A. the cleaning of substrate: first by the SiO of purchase2/ Si substrate, which is put into toluene solution, to be cleaned by ultrasonic 10 minutes, then is put
Enter to be cleaned by ultrasonic in acetone soln 10 minutes, then with being cleaned by ultrasonic 10 minutes in deionized water, place into dehydrated alcohol water
Ultrasonic cleaning 10 minutes, finally dries up substrate.
B. prepared by thermosensitive film: using magnetron sputtering method by Mn1.56Co0.96Ni0.48Alloy target material is splashed to obtained by step a
Substrate on, sputtering condition are as follows: basic air pressure 6x10-4Pa, operating air pressure 2Pa, sputter gas high-purity Ar gas, sputtering power
100W, 10 DEG C of underlayer temperature.
C. it makes annealing treatment: the Mn-Co-Ni film that step b is obtained is put into high-temperature electric resistance furnace, be arranged 900 DEG C of temperature, heat preservation
Time 120 minutes, heating and rate of temperature fall were all 5 DEG C/min, obtained Mn-Co-Ni-O film.
D. prepared by electrode: using the method for evaporation coating in the silver-plated interdigital electrode of Mn-Co-Ni-O film surface.Interdigital length
Degree is 6.2mm, width 0.8mm.
Measure the room temperature resistance R of Mn-Co-Ni-O thermosensitive film in the embodiment25For 147.5k Ω, temperature-sensitive constant B value is
3385K。
R25, constant B value in above-described embodiment etc., are all satisfied the usual definition of negative temperature coefficient thermistor composition；Wherein,
R25 is room temperature resistance, also known as normal resistance, refers to the zero-power resistance measured at 25 DEG C；Temperature-sensitive constant B value is two temperature
Under the ratio of the difference of the difference of the natural logrithm of zero-power resistance and the two inverse temperatures that measures, that is to say, that B=[ln
(RT1/RT2)]/[(1/T1)-(1/T2)]。
Above-described embodiment is only to prepare Mn-Co-Ni-O system (also system containing Mn-Co-Ni-Cu-O) negative temperature coefficient heat-sensitive film
For, using alloy target material first sputters re-annealing, the method for oxidation is equally applicable to other negative temperature coefficient heat-sensitives in the present invention
System, such as Mn-Ni-O series negative temperature coefficient thermosensitive film, Mn-Fe-Ni-O series negative temperature coefficient thermosensitive film.Correspondingly, when system
When standby Mn-Ni-O series negative temperature coefficient thermosensitive film, thermosensitive film preparation is to use magnetron sputtering method by Mn-Ni alloy target material
(its alloying component of target is mainly made of Mn element and Ni element) is splashed on substrate, using annealing；As preparation Mn-
When Fe-Ni-O series negative temperature coefficient thermosensitive film, thermosensitive film preparation is to use magnetron sputtering method by Mn-Fe-Ni system alloys target
Material (its alloying component of target is mainly made of Mn element, Fe element and Ni element) is splashed on substrate, using annealing；
Condition setting, parameter setting used by magnetron sputtering method, annealing atmosphere used by making annealing treatment, annealing time, annealing temperature
Degree etc., can with prepare the identical of Mn-Co-Ni-O series negative temperature coefficient thermosensitive film.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (8)
1. a kind of preparation method of negative temperature coefficient heat-sensitive film, which comprises the following steps:
(1) cleaning of substrate；
(2) prepared by thermosensitive film: Mn-Co-Ni alloy target material being splashed to gained after step (1) is cleaned using magnetron sputtering method
Drying substrate on, obtain Mn-Co-Ni system film；Wherein, condition used by the sputtering are as follows: basic air pressure < 1x10- 4Pa, sputter gas are the high-purity Ar gas that purity is not less than 99.9%, and sputtering power meets 80-120W, underlayer temperature 100-
250℃；
(3) it makes annealing treatment: the resulting Mn-Co-Ni system film of step (2) is carried out at anneal oxidation under the atmosphere containing oxygen
Mn-Co-Ni-O system film is prepared in reason, and the Mn-Co-Ni-O system film, that is, Mn-Co-Ni-O series negative temperature coefficient temperature-sensitive is thin
Film；Wherein, it is 600-900 DEG C that the anneal oxidation, which handles used annealing temperature, and annealing soaking time is 90-150 minutes.
2. the preparation method of negative temperature coefficient heat-sensitive film as described in claim 1, which is characterized in that in the step (2), institute
Mn-Co-Ni alloy target material its alloying component is stated mainly to be made of Mn element, Co element and Ni element.
3. the preparation method of negative temperature coefficient heat-sensitive film as claimed in claim 2, which is characterized in that in the step (2), institute
Its alloying component of Mn-Co-Ni alloy target material is stated to be made of Mn element, Co element and Ni element；Correspondingly, the step (3)
Mn-Co-Ni-O system film obtained is specially Mn-Co-Ni-O film.
4. the preparation method of negative temperature coefficient heat-sensitive film as claimed in claim 2, which is characterized in that in the step (2), institute
Stating in its alloying component of Mn-Co-Ni alloy target material further includes Cu element, correspondingly, the Mn- made from the step (3)
Co-Ni-O system film is specially Mn-Co-Ni-Cu-O film.
5. the preparation method of negative temperature coefficient heat-sensitive film as described in claim 1-4 any one, which is characterized in that the step
Suddenly in (3), the anneal oxidation processing carries out in air atmosphere.
6. the preparation method of negative temperature coefficient heat-sensitive film as described in claim 1-5 any one, which is characterized in that described negative
The preparation method of temperature coefficient thermal film is further comprising the steps of:
(4) electrode is prepared: the Mn-Co-Ni-O system film surface obtained using the method for evaporation coating in the step (3)
Prepare interdigital electrode.
7. a kind of preparation method of negative temperature coefficient heat-sensitive film, which comprises the following steps:
(1) cleaning of substrate；
(2) thermosensitive film prepare: using magnetron sputtering method by Mn-Ni alloy target material be splashed to step (1) cleaning after it is resulting
On dry substrate, Mn-Ni system film is obtained；Wherein, condition used by the sputtering are as follows: basic air pressure < 1x10-4Pa splashes
Body of emanating is the high-purity Ar gas that purity is not less than 99.9%, and sputtering power meets 80-120W, and underlayer temperature is 100-250 DEG C；
(3) it makes annealing treatment: the resulting Mn-Ni system film of step (2) is subjected to anneal oxidation processing under the atmosphere containing oxygen
Mn-Ni-O system film is prepared, the Mn-Ni-O system film, that is, Mn-Ni-O series negative temperature coefficient thermosensitive film；Wherein, described
Annealing temperature used in anneal oxidation processing is 600-900 DEG C, and annealing soaking time is 90-150 minutes.
8. a kind of preparation method of negative temperature coefficient heat-sensitive film, which comprises the following steps:
(1) cleaning of substrate；
(2) prepared by thermosensitive film: Mn-Fe-Ni alloy target material being splashed to gained after step (1) is cleaned using magnetron sputtering method
Drying substrate on, obtain Mn-Fe-Ni system film；Wherein, condition used by the sputtering are as follows: basic air pressure < 1x10- 4Pa, sputter gas are the high-purity Ar gas that purity is not less than 99.9%, and sputtering power meets 80-120W, underlayer temperature 100-
250℃；
(3) it makes annealing treatment: the resulting Mn-Fe-Ni system film of step (2) is carried out at anneal oxidation under the atmosphere containing oxygen
Mn-Fe-Ni-O system film is prepared in reason, and the Mn-Fe-Ni-O system film, that is, Mn-Fe-Ni-O series negative temperature coefficient temperature-sensitive is thin
Film；Wherein, it is 600-900 DEG C that the anneal oxidation, which handles used annealing temperature, and annealing soaking time is 90-150 minutes.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110106485A (en) * | 2019-05-18 | 2019-08-09 | 中国科学院新疆理化技术研究所 | A kind of negative temperature coefficient heat-sensitive film and preparation method thereof |
| CN112663002A (en) * | 2020-09-04 | 2021-04-16 | 中科传感(佛山)科技有限公司 | Thermistor film preparation method based on direct-current reactive co-sputtering |
| CN112735709A (en) * | 2020-12-26 | 2021-04-30 | 广东工业大学 | Film type negative temperature coefficient sensor and preparation method thereof |
| CN114134457A (en) * | 2021-12-07 | 2022-03-04 | 中国科学院新疆理化技术研究所 | Preparation method of composite NTC thermosensitive film with grating-like structure |
| CN114150266A (en) * | 2021-12-02 | 2022-03-08 | 西安文理学院 | Preparation method of molybdenum disulfide film |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020010347A (en) * | 2000-07-29 | 2002-02-04 | 문창호 | Thermistor with multi function and the manufacturing method |
| CN104439245A (en) * | 2013-09-17 | 2015-03-25 | 无锡慧明电子科技有限公司 | Method for preparing single-orientation thermosensitive thin film through vacuum coating |
| CN107622851A (en) * | 2017-09-25 | 2018-01-23 | 江苏时瑞电子科技有限公司 | A kind of negative tempperature coefficient thermistor with nano-particular film and preparation method thereof |
| CN107881475A (en) * | 2016-09-30 | 2018-04-06 | 江西理工大学 | A kind of method that Ni Co Mn Ti alloy firms are prepared by magnetron sputtering DC sputturing method |
-
2019
- 2019-02-27 CN CN201910145223.XA patent/CN109735807B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020010347A (en) * | 2000-07-29 | 2002-02-04 | 문창호 | Thermistor with multi function and the manufacturing method |
| CN104439245A (en) * | 2013-09-17 | 2015-03-25 | 无锡慧明电子科技有限公司 | Method for preparing single-orientation thermosensitive thin film through vacuum coating |
| CN107881475A (en) * | 2016-09-30 | 2018-04-06 | 江西理工大学 | A kind of method that Ni Co Mn Ti alloy firms are prepared by magnetron sputtering DC sputturing method |
| CN107622851A (en) * | 2017-09-25 | 2018-01-23 | 江苏时瑞电子科技有限公司 | A kind of negative tempperature coefficient thermistor with nano-particular film and preparation method thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110106485A (en) * | 2019-05-18 | 2019-08-09 | 中国科学院新疆理化技术研究所 | A kind of negative temperature coefficient heat-sensitive film and preparation method thereof |
| CN110106485B (en) * | 2019-05-18 | 2021-04-27 | 中国科学院新疆理化技术研究所 | Negative temperature coefficient thermosensitive film and preparation method thereof |
| CN112663002A (en) * | 2020-09-04 | 2021-04-16 | 中科传感(佛山)科技有限公司 | Thermistor film preparation method based on direct-current reactive co-sputtering |
| CN112735709A (en) * | 2020-12-26 | 2021-04-30 | 广东工业大学 | Film type negative temperature coefficient sensor and preparation method thereof |
| CN114150266A (en) * | 2021-12-02 | 2022-03-08 | 西安文理学院 | Preparation method of molybdenum disulfide film |
| CN114134457A (en) * | 2021-12-07 | 2022-03-04 | 中国科学院新疆理化技术研究所 | Preparation method of composite NTC thermosensitive film with grating-like structure |
| CN114134457B (en) * | 2021-12-07 | 2023-11-24 | 中国科学院新疆理化技术研究所 | Preparation method of grating-like structure composite NTC thermosensitive film |
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